Sodium Iodide → HCID 70391052、化合物

HRID 621031ノート

反応式

HRID 621031 の反応式
[CH3:1][O:2][C:3]1[CH:36]=[C:35]([O:37][CH3:38])[CH:34]=[CH:33][C:4]=1[CH2:5][N:6]1[C@H:9]([CH2:10]OS(C2C=CC(C)=CC=2)(=O)=O)[C@H:8]([NH:22][C:23](=[O:31])[CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:7]1=[O:32].[I-:39].[Na+]>CC(C)=O>[CH3:1][O:2][C:3]1[CH:36]=[C:35]([O:37][CH3:38])[CH:34]=[CH:33][C:4]=1[CH2:5][N:6]1[C@H:9]([CH2:10][I:39])[C@H:8]([NH:22][C:23](=[O:31])[CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:7]1=[O:32]

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 86740463HCID 86740463、化合物

生成物 1

HCID 70391052HCID 70391052、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To 70 ml of acetone was added 2.27 g of cis-1-(2,4-dimethoxybenzyl)-3-phenylacetamido-4-(p-toluenesulfonyloxymethyl)-2-oxoazetidine and 4.95 g of sodium iodide, and the mixture is heated under reflux for 6 hours with stirring, and then concentrated in vacuo. To the residue are added methylene chloride and water to dissolve it, and the methylene chloride layer is separated and washed successively with an aqueous sodium thiosulfate solution and an aqueous sodium chloride solution. The methylene chloride layer is then dried over magnesium sulfate and the solvent is distilled off in vacuo. Ethyl acetate is added to the residue and the precipitated crystals are collected by filtration to give cis-1-(2,4-dimethoxybenzyl)-4-iodomethyl-3-phenylacetamido-2-oxoazetidine, m.p. 181°-182° C.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 6 hours
  3. concentrationconcentrated in vacuo
  4. additionTo the residue are added methylene chloride and water
  5. dissolutionto dissolve it
  6. customthe methylene chloride layer is separated
  7. washwashed successively with an aqueous sodium thiosulfate solution
  8. dry with materialThe methylene chloride layer is then dried over magnesium sulfate
  9. distillationthe solvent is distilled off in vacuo
  10. additionEthyl acetate is added to the residue
  11. filtrationthe precipitated crystals are collected by filtration

出典と根拠

ORDレコード
ord-75a0f7f8f86a49a1b7d00d1246224293
出典データセット
uspto-grants-1989_04
特許番号
US04822790

反応ノート

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